CN112129802B - Quantitative analysis method for pore volume increment of hydrated shale in different scales - Google Patents
Quantitative analysis method for pore volume increment of hydrated shale in different scales Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N24/00—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects
- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
- G01N24/081—Making measurements of geologic samples, e.g. measurements of moisture, pH, porosity, permeability, tortuosity or viscosity
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N15/088—Investigating volume, surface area, size or distribution of pores; Porosimetry
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract
The invention belongs to the technical field of oil and gas exploration and development, and particularly relates to a quantitative analysis method for pore volume increment of hydrated shale in different scales. According to the quantitative analysis method for the increment of the pore volume of the hydrated shale in different scales, the first solvent which does not generate hydration reaction with the shale is adopted to saturate a standard rock sample, the original effective pore volume data is obtained through testing, and then the water is adopted to perform saturation testing, so that the real variation data of the pores in different scales after the hydration of the shale can be obtained. The method can realize quantitative evaluation of absolute increase amplitude of effective pore volumes of different scales in shale under hydration, and has practical significance for guiding on-site screening of shale reservoirs suitable for production increase after well-logging.
Description
Technical Field
The invention belongs to the technical field of oil and gas exploration and development, and particularly relates to a quantitative analysis method for pore volume increment of hydrated shale in different scales.
Background
Shale is an important unconventional natural gas resource, and the exploration and development of shale gas can greatly relieve the pressure of natural gas demand and improve the energy structure and energy safety. Hydraulic fracturing is one of the key technologies for successful development of shale gas reservoirs. Unlike conventional hydrocarbon reservoirs, field experience has proven that some shale gas well reservoirs are hydraulically fractured and then shut in for a period of time (i.e., post-fracturing "kill" stage), and the flowback fracturing fluid can effectively improve the shale gas well productivity. The "kill" stimulation mechanism of shale gas wells is currently not completely understood. One explanation is that during "snuffing" hydration reactions occur due to the fracturing fluid coming into full contact with the shale, increasing the effective porosity of the shale reservoir and enhancing the seepage capability of the reservoir gas, thereby achieving increased production. But currently there is no method for quantitatively evaluating the magnitude of shale porosity increase upon hydration.
In order to research the yield increasing mechanism of shale gas well "dead well", in the prior art, a nuclear magnetic resonance quantitative detection method for shale microcrack damage is related, and although the nuclear magnetic resonance method is used for quantitatively analyzing the microcrack damage of the rock under the hydration, the disadvantage of the method is that T 2 The increment of the spectral area consists of two parts: the amount of distilled water imbibed into the core and the amount of increase in the core's pore space within the time interval. So it cannot be directly considered as T 2 The increment of the spectrum area is the increment of the pore in the core. Therefore, the method cannot evaluate the absolute increase amplitude of the pore spaces of different scales of shale cores under the hydration effect, but the absolute increase amplitude of the pore spaces of different scales directly influences whether the shale gas well is suitable for "dead well" production increase after pressing.
In the prior art, a shale hydration damage test method based on CT scanning is also involved, and the shale damage under hydration is quantitatively analyzed by utilizing a CT scanning means. However, this method has the disadvantage that the total pore volume (including the effective pore volume and the ineffective pore volume) of the core is obtained by CT scanning. But only the effective pore volume contributes to shale gas production. In addition, hydration may convert ineffective pore connectivity into effective pores. However, CT scanning cannot identify this situation, and CT scanning can only identify the newly added pore volume.
In summary, the test method related to shale pore variation in the prior art cannot accurately reflect the influence of the "well-logging" operation on pores of different scales, so that shale gas wells suitable for increasing the yield of the "well-logging" after being pressed cannot be accurately screened.
Disclosure of Invention
Therefore, the invention aims to overcome the defects that the test method for shale pore change in the prior art cannot accurately reflect the influence of the 'well-stewed' operation on the pore and cannot accurately guide actual production and the like, and further provides a quantitative analysis method for the volume increment of the pores of the hydrated shale with different dimensions.
Therefore, the invention provides the following technical scheme:
the invention provides a quantitative analysis method for pore volume increment of hydrated shale with different dimensions, which comprises the following steps,
(1) Determination of the T of the unitary quality of water and first solvent Using Nuclear magnetic resonance 2 Spectral signal according to T 2 Determining a conversion coefficient by the spectrum semaphore; calibrating nuclear magnetic resonance T corresponding to unit volume of first solvent and water 2 Spectral semaphore S 1 And S is 2 ，
Wherein the first solvent is a solvent which does not react with shale in a hydration way;
(2) Preparing a standard rock sample of a target shale area, drying and cooling to room temperature;
(3) Completely saturating the standard rock sample by adopting a first solvent, and performing nuclear magnetic resonance scanning on the standard rock sample to obtain T 2 Spectrum A 1 The conversion coefficient obtained according to the step (1) is corrected to be A 1 ’，A 1 ' total integral area is a 1 ' wherein the first peak integration area is a p1 The second peak integral area is a p2 ；
(4) Drying standard rock sample, cooling to room temperature, and performing nuclear magnetic resonance scanning to obtain T 2 Spectrum A 2 ，A 2 Total integral area is a 2 ；
(5) Completely saturating the standard rock sample with water, and performing nuclear magnetic resonance scanning on the standard rock sample to obtain T 2 Spectrum B 1 ，B 1 Integral area b 1 Wherein the first peak integration area is b p1 The second peak integral area is b p2 ；
(6) Drying standard rock sample, cooling to room temperature, and performing nuclear magnetic resonance scanning to obtain T 2 Spectrum B 2 ，B 2 Total integral area b 2 ；
(7) The data is calculated and the data is obtained,
original effective void volume V of rock sample 0 The method comprises the following steps:
the first peak corresponds to the small effective pore volume, V 0S The method comprises the following steps:
the second peak corresponds to the large effective pore volume, the original large effective pore volume V 0L The method comprises the following steps:
effective pore volume V of rock sample after hydration T The method comprises the following steps:
the first peak corresponds to the small-size effective pore, and the small-size effective pore volume V after hydration TS The method comprises the following steps:
the second peak corresponds to the large-size effective pore, and the large-size effective pore volume V after hydration TL The method comprises the following steps:
optionally, the first solvent is any one of absolute ethyl alcohol or silicone oil.
Optionally, the first solvent is absolute ethanol.
Optionally, the temperature of the drying is 75-85 ℃ and the time is 5-7 h.
Optionally, the temperature of the drying is 80 ℃ and the time is 6 hours.
Alternatively, the standard rock sample has dimensions Φ25×50mm.
Alternatively, T of the water and the first solvent 2 T of the conversion coefficients of the spectrum signals 2 Ratio of spectral wave signal quantity.
Optionally, the demarcation point of the pore diameters of the small-size effective pore and the large-size effective pore is T 2 The troughs of the spectral peak signal.
T of shale core 2 The spectrum shows a bimodal characteristic, the lowest point between two peaks is the demarcation point of the two peaks, as shown in fig. 2, the left peak corresponds to a small-size pore, and the right peak corresponds to a large-size pore.
Optionally, the standard rock sample is fully saturated by means of vacuumizing and saturation.
The quantitative analysis method for the volume increment of the pores of the hydrated shale with different dimensions provided by the invention has the following working principle: the hydrogen signal in a rock sample comes mainly from three parts: free water, bound water, clay bound water. Wherein free water and bound water occupy void space, and clay bound water does not occupy void space. The purpose of drying the rock sample at 80 ℃ for 6 hours after the rock sample is prepared is to remove free water and bound water in the rock sample (the free water and the bound water occupy pore space; the clay bound water does not occupy the pore space, so that the clay bound water does not need to be removed), and errors on test results are prevented. The nuclear magnetic scanning is carried out after the rock sample is saturated with absolute ethyl alcohol so as to obtain the original pore volume of the rock sample. The drying at 80 ℃ for 6 hours is to remove the absolute ethyl alcohol in the rock sample and prepare for the subsequent operation. The nuclear magnetic scanning is performed again to acquire signals of the part of the clay in the rock sample, which is bound with water, in the current state. The clay bound water, because it does not occupy the pore space, needs to be subtracted from this signal value in the later calculations. The nuclear magnetic scanning is carried out after the rock sample is saturated with deionized water so as to obtain the pore volume of the rock sample after hydration. The drying at 80 ℃ for 6 hours was to remove deionized water from the rock sample. The nuclear magnetic scanning is performed again to acquire signals of the part of the clay in the rock sample, which is bound with water, in the current state. The clay bound water, because it does not occupy the pore space, needs to be subtracted from this signal value in the later calculations. Thus, the real data of the variation of the pores with different dimensions after the shale hydration can be obtained.
The technical scheme of the invention has the following advantages:
1. according to the quantitative analysis method for the increment of the pore volume of the hydrated shale in different scales, the first solvent which does not generate hydration reaction with the shale is adopted to saturate a standard rock sample, the original effective pore volume data is obtained through testing, and then the water is adopted to perform saturation testing, so that the real variation data of the pores in different scales after the hydration of the shale can be obtained. The method can realize quantitative evaluation of absolute increase amplitude of effective pore volumes of different scales in shale under hydration, and has practical significance for guiding on-site screening of shale reservoirs suitable for production increase after well-logging. According to the invention, through the first study, when the increase of the effective pore volume of the target reservoir shale is obvious, the hydration effect generated in the process of 'well-flushing' can effectively improve the effective pore volume of the reservoir and improve the seepage capability of gas, so that the productivity of a gas well is improved, and the target shale reservoir is suitable for 'well-flushing'; when the increase of the small-size effective pore volume of the shale of the target reservoir is obvious, but the increase of the large-size effective pore volume is not obvious, the hydration in the process of 'soaking the well' is shown to improve the effective pore volume of the reservoir, but the seepage capability of gas in the reservoir is not effectively improved, and the capacity of a gas well is increased to a limited extent, so that the target shale reservoir is carefully selected to be subjected to 'soaking the well'; when the increase in effective pore volume is not significant for both small and large shale sizes of the target reservoir, then the target shale reservoir is not suitable for "snubbing".
2. According to the quantitative analysis method for the volume increment of the hydrated shale pores with different dimensions, provided by the invention, ethanol is adopted as the first solvent, and the standard rock sample is easy to dry and has no residue in the testing process, so that the testing result is more accurate.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is a nuclear magnetic resonance spectrum of a rock sample 1 in example 1 of the present invention;
FIG. 2 is T of FIG. 1 2 Spectrum B 2 Spectrograms in different coordinate systems.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides a quantitative analysis method for pore volume increment of hydrated shale with different dimensions, which comprises the following specific steps:
1. determination of unit mass (1 g) of Water and absolute ethanol T by Nuclear magnetic resonance 2 Spectrum, T 2 The amplitude values of the spectrum signals are 915 and 1182 respectively, and the conversion coefficients of the spectrum signals and 1182 are determined to be 1:1.3; the corresponding signal quantity of absolute ethyl alcohol and water of a calibrated unit volume (1 mL) is S respectively 1 And S is 2 . The experiment is calibrated to be anhydrous in unit volumeThe corresponding signal quantity of ethanol and water is S respectively 1 = 24472 and S 2 ＝28623。
2. The standard rock sample of the target shale area is prepared by adopting a linear cutting mode, in the embodiment, the shale rock sample is from three different shale gas wells in Yuxi Yongchuan area, the numbers of the shale rock sample are respectively 1# and 2# and 3# and the sizes of the shale rock sample are phi 25 multiplied by 50mm. Then drying the rock sample at 80 ℃ for 6 hours;
3. after the rock sample is cooled to room temperature, completely saturating the rock sample in a vacuumizing saturation mode, wherein saturated liquid is absolute ethyl alcohol;
4. after saturation is completed, performing nuclear magnetic resonance scanning on the rock sample to obtain T 2 Spectrum A 1 Correction (T 2 The amplitude value of the spectrum signal is divided by 1.3) to be A 1 ’，A 1 ' total integral area is a 1 ' wherein the first peak has an integrated area of a p1 The second peak integral area is a p2 ；
5. Drying the rock sample at 80 ℃ for 6 hours, cooling to room temperature, and performing nuclear magnetic resonance scanning on the rock sample to obtain T 2 Spectrum A 2 ，A 2 Total integral area is a 2 。
6. Completely saturating the rock sample in a vacuumizing saturation mode, wherein saturated liquid is deionized water;
7. after saturation is completed, performing nuclear magnetic resonance scanning on the rock sample to obtain T 2 Spectrum B 1 ，B 1 Integral area b 1 Wherein the first peak integration area is b p1 The second peak integral area is b p2 ；
8. Drying the rock sample at 80 ℃ for 6 hours, cooling to room temperature, and performing nuclear magnetic resonance scanning on the rock sample to obtain T 2 Spectrum B 2 ，B 2 Integral area b 2 . The specific test results are shown in Table 2.
9. And (3) data calculation:
since absolute ethanol does not hydrate with shale, the volume of alcohol entering the rock sample can be considered as the original effective void volume of the rock sample as:
the first peak corresponds to small-size effective pores, the original small-size effective pore volume is:
the second peak corresponds to large-size effective pores, the original large-size effective pore volume is:
after the deionized water entering the rock sample and shale are hydrated, the effective pores in the rock sample are filled, and the volume of the deionized water can be regarded as the effective pore volume of the rock sample after hydration:
the first peak corresponds to small-size effective pores, and the small-size effective pore volume after hydration is:
the second peak corresponds to large-size effective pores, and the large-size effective pore volume after hydration is:
the nuclear magnetic resonance spectrum of the 1# experimental rock sample tested in this example is shown in fig. 1, the spectrum area integration results are shown in the following table,
TABLE 1
According to the above formula, the results of calculating various effective pore volumes are shown in the following table, wherein the permeability test method is as follows:
the permeability test method is used for GB/T34533-2017 'determination of porosity and pulse attenuation method permeability of shale helium method'.
TABLE 2
From the experimental results, when the effective pore volume of the target reservoir shale is obviously increased in the small-size and large-size, the hydration generated in the process of "soaking well" can effectively improve the effective pore volume of the reservoir and improve the seepage capability of gas so as to increase the productivity of a gas well, and the target shale reservoir is suitable for "soaking well" (according to the Darcy formula, the permeability of the reservoir is in direct proportion to the shale gas yield, the greater the permeability of the reservoir is, the higher the yield is, and the core permeability 1 in the table is obviously increased); when the increase of the small-size effective pore volume of the shale of the target reservoir is obvious, but the increase of the large-size effective pore volume is not obvious, the hydration in the process of 'soaking well' is shown to improve the effective pore volume of the reservoir, but the seepage capability of gas in the reservoir is not effectively improved, and the productivity of a gas well is limited, so that the target shale reservoir is carefully selected to be subjected to 'soaking well' (the increase of the permeability of a core No. 2 in the table is limited); when the increase of the effective pore volume of the shale of the target reservoir is not obvious, the shale of the target reservoir is not suitable for "braising" (the permeability of the core No. 3 in the table is almost unchanged). According to the method, quantitative analysis is carried out on the pore volume increment of different scales of shale after hydration (well logging) for the first time through nuclear magnetic resonance, and whether the shale gas well is suitable for the operation of well logging after pressing is accurately judged according to the pore volume increment of different scales, so that the method has more direct guiding significance on actual production.
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. And obvious variations or modifications thereof are contemplated as falling within the scope of the present invention.
Claims (8)
1. A quantitative analysis method for the volume increment of pores of hydrated shale with different dimensions is characterized by comprising the following steps,
(1) Determination of the T of the unitary quality of water and first solvent Using Nuclear magnetic resonance 2 Spectral signal according to T 2 Determining a conversion coefficient by the spectrum semaphore; calibrating nuclear magnetic resonance T corresponding to unit volume of first solvent and water 2 Spectral semaphore S 1 And S is 2 ，
Wherein the first solvent is a solvent which does not react with shale in a hydration way; t of the water and the first solvent 2 T of the conversion coefficients of the spectrum signals 2 A ratio of spectral wave signal quantities;
(2) Preparing a standard rock sample of a target shale area, drying and cooling to room temperature;
(3) Completely saturating the standard rock sample by adopting a first solvent, and performing nuclear magnetic resonance scanning on the standard rock sample to obtain T 2 Spectrum A 1 The conversion coefficient obtained according to the step (1) is corrected to be A 1 ’，A 1 ' total integral area is a 1 ' wherein the first peak integration area is a p1 The second peak integral area is a p2 The method comprises the steps of carrying out a first treatment on the surface of the The correction method is to make T 2 Spectral signal amplitude value A 1 Multiplying the conversion coefficient;
(4) Drying standard rock sample, cooling to room temperature, and performing nuclear magnetic resonance scanning to obtain T 2 Spectrum A 2 ，A 2 Total integral area is a 2 ；
(5) Completely saturating the standard rock sample with water, and performing nuclear magnetic resonance scanning on the standard rock sample to obtain T 2 Spectrum B 1 ，B 1 Integral area b 1 Wherein the first peak integration area is b p1 The second peak integral area is b p2 ；
(6) Drying standard rock sample, cooling to room temperature, and performing nuclear magnetic resonance scanning to obtain T 2 Spectrum B 2 ，B 2 Total integral area b 2 ；
(7) The data is calculated and the data is obtained,
original effective void volume V of rock sample 0 The method comprises the following steps:
the first peak corresponds to the small effective pore volume, V 0S The method comprises the following steps:
the second peak corresponds to the large effective pore volume, the original large effective pore volume V 0L The method comprises the following steps:
effective pore volume V of rock sample after hydration T The method comprises the following steps:
the first peak corresponds to the small-size effective pore, and the small-size effective pore volume V after hydration TS The method comprises the following steps:
the second peak corresponds to the large-size effective pore, and the large-size effective pore volume V after hydration TL The method comprises the following steps:
2. the method for quantitatively analyzing the different-scale pore volume increment of the hydrated shale according to claim 1, wherein the first solvent is any one of absolute ethyl alcohol or silicone oil.
3. The method of quantitatively analyzing different scale pore volume increments of hydrated shale of claim 2, wherein the first solvent is absolute ethanol.
4. A method for quantitative analysis of different scale pore volume increments of hydrated shale according to any of claims 1-3, wherein the temperature of the drying is 75-85 ℃ for a period of 5-7 hours.
5. The method for quantitatively analyzing the increment of the pore volume of the hydrated shale with different scales as recited in claim 4, wherein the temperature of the drying is 80 ℃ and the time is 6 hours.
6. The method of quantitatively analyzing the different scale pore volume increments of hydrated shale of claim 4, wherein the standard rock sample has dimensions Φ25×50mm.
7. The quantitative analysis method for the increment of the pore volume of the hydrated shale with different dimensions according to claim 4, wherein the demarcation point of the pore diameters of the small-size effective pores and the large-size effective pores is T 2 The troughs of the spectral peak signal.
8. The method for quantitatively analyzing the pore volume increment of the hydrated shale with different scales according to any one of claims 1 to 3 or 5 to 7, wherein the standard rock sample is fully saturated in a vacuum saturation mode.
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